Chinese Journal of Chromatography ›› 2016, Vol. 34 ›› Issue (6): 615-620.DOI: 10.3724/SP.J.1123.2016.03015

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Determination of migratory organotin compounds in toys by headspace-solid phase microextraction coupled with gas chromatography-mass spectrometry

HUO Juyuan1,2, OUYANG Gangfeng2, CHEN Liqiong1, WANG Xin1   

  1. 1. Shenzhen Academy of Metrology and Quality Inspection, Shenzhen 518109, China;
    2. School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275, China
  • Received:2016-03-10 Online:2016-06-08 Published:2013-01-23
  • Supported by:

    Scientific Research Fund of Shenzhen Academy of Metrology and Quality Inspection (No. 2015-YN12).

Abstract:

A method for the determination of ten migratory organotin compounds in toys was developed using headspace-solid phase microextraction (HS-SPME) coupled with gas chromatography-mass spectrometry (GC-MS). Toy materials were soaked in 0.07 mol/L HCl for 2 h, then the pH of the soak solution was adjusted to 4.7 by HAc-NaAc buffer. After ethylized with sodium tetraethylborate (NaBEt4), the soaked solution was agitated and the headspace solid phase microextraction was performed with a 100 μ m polydimethylsiloxane (PDMS) fiber. After extraction, the SPME fiber was directly injected into the GC inlet, and the organotin compounds were separated on a DB-5 capillary column. The limits of detection for the ten organotin compounds were in the range of 0.5-5 μg/kg. The recoveries were in the ranges of 80.7%-118.7% and 86.2%-120.5% at the spiked levels of 0.500 μg/L and 5.00 μg/L. The relation standard deviations (RSDs) were all less than 15%. This method has been used to determine migratory organotin in accessible parts of toys, including coating, plastic, wood and textile. The method is simple, fast, sensitive and solvent-free.

Key words: gas chromatography-mass spectrometry (GC-MS), headspace-solid phase microextraction (HS-SPME), organotin compounds, toys

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